Process of treatment of vinasses.



PATENTED JAN. 23, 1906.

.c. SUDRE.

PROCESS OF TREATMENT OF VINASSES.

APPLICATIONIILEITJAN. e, 1904. RENEWED NOV. 7, 1905.

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lengt UNITED STATES PATENT OFFICE.

Specification of Letters Patent.

' Patented Jan. 23, 1906 Original application filed December 80,1902, Serial No. 187,127. Divided and this application filed January 6, 1904. Renewed November 7, 1905. Serial No. 286,288.

To all whom it may concern:

Be it known that I, CHARLES SUDRE, of No. 33 Boulevard Haussmann,Paris, France, have invented a certain new and useful Process of Treatment of Vinasses; and I do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same.

This ap lication is a division of a prior application ed by me on the 30th day of December, 1902, Serial No. 137,127.

. Up to the present in any process for treating the res'iduary liquors of the distillation of the syrup of beet-roots called vinasses in order to extract from them glycerin and other useful products some mechanical apparatus for scraping or cleaning the exhausted products has always had to be employed.

By reason of the very construction of any previous apparatus numerous by-products are produced, which pass into the distilled liquid and render it very impure. It is well known that in order to extract the glycerin without decomposition it is necessary to work in as complete a vacuum as possible. The vinasses under the action of heat and in a vacuum first of all distils water and a little glycerin, when the material becominganhydrous it distils the rest of the glycerin. During the first part of the operation the steam becoming disengaged produces 'a froth and carries numerous particles which hinder the operations and in many of the processes used up to now render the working impossible if the vinasses are viscous.

The process which is the subject of the present application for a patent does away with this inconvenience. It is based on the following discoveries and appliances:

First. If the vinasses from a distillery (of treacle, for example) be distilled in a vacuum at a temperature of not more than 300, the residue after the g1 cerin and the water have been extracted, is liquid at this temperature of 300 and flows away of its own accord. The gycerin and water are extracted in a 'of time which depends on thethickness of the'vinasses. My process consists, in principle, of providing along the'walls of an inclosure, suitably arranged, in which there is a vacuum and which is heated by some exteriorsource of-heat in such a way that the temperature of the walls cannot be greater than 300, a constant stream of the vinasses of regular and regulated thickness. Thus the vinasses enter and pour away in a continuous liquid state without the intervention of any mechanical apparatus and lose in their passage (supposing that this is of a length suitable to the thickness of the liquid film) first'of all the water and then the glycerin.

Second. It is proved that if the vinasses are sufiicientl acidulated the ammonia escapes only in iniinitesimal proportions and remains concentrated in the residue.

Third. By forcin the vapors to take up in the a paratus itsef a rapid gyratory helicoidamovement I obtain b centrifugal force the impin ement against tl ie heated walls of the partifies carried by the vapors, which partlcles thereby have a fresh opportunity of eing distilled.

Fourth. It'is admitted that it'is necessary to have a current of, superheated steam to help the distillation of the glycerin when the vinasses have become anhydrous. In many processes this steam is introduced from without and on condensing produces a dilute mixture of water and glycerin. On the contrary I utilize for this purpose the steam arisin from the vinasse itself, which is superheate in the apparatus while taking up its gyratory movement. The superheated steam then bathes and surrounds, before it leaves the apparatus, the glycerin which is given off by the anhydrous substance and draws it out of the distilling apparatus. The glycerin and water vapors exhausted by a pump are condensed into a mixture of glycerin and water, which is concentrated for sale, and the liquid residue made solid by cold and. retaining all the ammonia is treated by some known means or sold as-it is;

These principles being set forth, I will describe as a representative example a construction for the carrying out of the process shown in section diagrammatically in the accompanying drawing and by which I put these rinc ples into practice; but it is evident hat the forms may be infinitely varied.

The ap aratus is designed to be heated by coke or cliarcoal, It consists of a distilling-. column a, formed of cast-iron tubes with or without exterior ribs, three to six meters high, according to the quantit of water in the vinasses to be treated. A ove this column is situated a distributer 1, which spreads stones through an annular passage onto the interior to 300 centigrade when the vinasses have surface of the column a continuous stream of the vinasses to be treated. At the foot of this column is placed a pipe 2 for the escape of the gas and vapors which are driven off by the vinasses under treatment. Below this the column is constricted and 'is terminated by a chamber 1;,- provided with sto -cocks c and d and in which the residue col acts and which is arranged in such a way that it can be drained off at regular intervals. Inside the column a is suspended or fastened in any convenient way a rod f, round which is coiled a helix 9, of which the outside surface is very close to the walls of the cast-iron column. The gas and vapors escape into a shorter accessory column h, called the purifying-column, smaller than the principal column, but also containing a fixed helix. The solid substances drawn in impin e onto the walls and, distilling g1 cerin whi e descending the whole length of t e walls, enter achamber like .the first, while the as and purified vapor are directed into a con enser i by a suction-pump 7c. The whole is inclosed wlthin a casing of refractory maternal 'm',leav1ng sufficient space between it and the column for the passa e ofthe gases for heating the apparatus. ese gases are produced in a furnace it, placed outside the column. This furnace is fed by coke or charcoal and is supplied with air by ablower o. The hot gases roceed by a vertical flue p to the top of the casing inclosing the column. In their passage a second blower g injects cold air into them in a regue lated quantity, so that their temperature at the top of the column is from 600 to 700 centigrade. The gases redescend in contact with the cast-iron column and produce the evaporation of the Water, whereby the greater portion of their heat is abstracted. About the middle of the column the ases are not more than 300 centi rade. The small column h annexed shou d not be higher than this point. As from other reasons the distillation of the rest of the glycerin, whichis in very small quantities, requires very little heat, the temperatureremains practically the same till it escapes by the lower flue.

The vinasses being watery and admitted to the vacuum, the water contained is distilled at 40 centigrade, and in consequence until all the water is distilled the temperature of the vinasses scarcely rises above this, in spite of the gases outside being at a temperature of 600 or 700 centigrade, all the heat of these being used up to d1stil the water. When the water is evaporated, the vinasses commence gradually to grow hotter, and after this time the gases must not rise beyond 300 centirade, or, as has been explained-before, the i fiuidity of the residue of the vinasses will be altered. The quantity and the temperature of the hot gases must, therefore, be regulated in such a way that their temperature is lowered lost all its water. This is why two blowers are used, of which the discharge can be regulated each independently of the other.

The steam produced inside and at the top of the column exhausted by the suctionpump is required to descend, which it does by following the path of the helix, taking up a gyratory movement, which by the centrifugal force developed ride it of all the particles which are thrown against the wall where thedistillation is completed, while descending the steam becomes superheated and helps in the distillation of the glycerin in the anh drous portions.

Let us now follow an operation. The vi nasses previously concentrated has some acid added to it, so as to have an acidity corresponding to 4 or 5 oil-1 50 Then it is introduced into the top of the column, which has first of all been brought up to the proper temperature by heating. The vinasses spread in a film and submitted to heat in a vacuum undergoes a violent ebullition. It'descends the length of the walls and loses first of all, as has been explained, its water, and then, becoming superheated, its glycerin. The steam in the upper portion, which contains particles in sus ension, enters the interior elix, the partic es under the action of centrifugal force are projected against the wall and further distilled, and, becoming heated, surround and draw the escaped glycerin first into the accessory column h, where it undergoes a fresh purification, then. into the condenser, where it again becomes liquid. The residuary gases after having been drawn. through the suction-pump are washed to rid them of any nitrogenous material they may contain, and then they escape into the atmosphere. The substances deposited in the accessory column undergo, as I have already described, a fresh distillation, and th glycerin they distil merges into the glycerinvapor from the principal column, which vapor passes through the accessory column. The substances deprived of glycerin l e": into the bottom chamber, from whence by means of successive movements of the stopcocks they are withdrawn at intervals. Thus by this apparatus is obtained,fi.rst, a mixture of glycerin and water of great purity, which has only to be concentrated to obtain glycerin ready for sale; second, a residuary liquid very hygrometric which solidifies in air, retaining all potash and nitrogen, which can be sold as it is for manure, or be redistilled with lime to produce ammonia, methylaniin, pyridie tars, or be treated in any other suitable man ner.

I claim.--

The herein-described process of extracting from vinasses the glycerin contained therein. in the form of a mixture of glycerin and water to be concentrated and for producing a residuo containing all the :immpnia which con- In Witness whereof I haye hereunto set my sists in first rendenng the vlnasses acid and .hand in presence of two wltnesses. [hen causing 1t t0 flow 1n a Vacuum alcng a CHARLES SUDRE surlmwu heated to a maximum temperature 5 of 300 Centigrade and causing the steam Witnesses:

produced to have a gyratory movementto LOUIS GARIDET, free it of pa-rtlclcs earned wlth 11;. r HERNANDO DE SOTO. 

